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Crystal Structure and Comparative Crystal Chemistry of AI2M~(OH)12(C03) · 3H20, a New Mineral from the Hydrotalcite-Manasseite Group A

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Crystal Structure and Comparative Crystal Chemistry of AI2M~(OH)12(C03) · 3H20, a New Mineral from the Hydrotalcite-Manasseite Group A Crystallography,Repons, Vol. 41, No.6, 1996, pp. 972-981. Transltnedfrom Kristallograjiya, VoL 41, No.6, 1996, pp. 1024-1034. @ Original Russian Text Copyright 1996 by Aralccheeva, Pushcharovskii, Rastwetaeva, Atencio, Luhman. Crystal Structure and Comparative Crystal Chemistry of AI2M~(OH)12(C03) · 3H20, a New Mineral from the Hydrotalcite-Manasseite Group A. v. Arakcheeva*, D. Yu. Pushcharovskii**, R. K. Rastsvetaeva***, D. Atencio****, and G. U. Lubman* Baikov Institute of Metallurgy, Russian Academy of Sciences, Leninskii pro 49, Moscow, 117334 Russia * Moscow State University, Moscow, 119899 Russia ** *** Shubnikov Institute of Crystallography, Russian Academy of Sciences, Leninskii pro 59, Moscow, //7333 Russia **** University of Sao Paulo, Sao Paulo, Brazil Received April 9, 1996 . 3H~O from Ihe Abstract-The crystal structure of a new mineral of the composition AI2Mg4(OH)12(C03) hydrotalcite-manasseite group has been determined by X-ray structure analysis. The parameters of Ihe hexag- onal unit cell are a =5.283(3), c = 15.150(9) A; sp. gr. P6 2m. The structure was refined over 52 cryslallograph- ically nonequivalent reflections up to R =0.039. The hydrogen atoms of hydroxyl groups are localized. The new mineral differs from otherrepresentatives oHhis group by the complete order of all the atoms, which is rctkl'!ed in a lower structure symmetry. The variety of minerals within the group is considered and interpreled in lerms of polytypism, the atomic order in the structure of sublattices, and isomorphous substitutions. INTRODUCTION Later on, one more mineral-chlormagaluminite (Mg, Fe)4A12(OH)dCI, (C03)o.sh 2H:O-w~ Depending on the composition of the octahedral included into the hydrotalcite-manasseite ..ubgroup. brucite-type cationic layers composing the structures of The hypothetical structure model of this mineral admits a very large group of natural and synthetic compounds the ordered arrangement of Al atoms in the (Mg, Fe, (the so-called dihydroxides), one can distinguish three AI3+, A1)-octahedra of a brucite layer [5]. The mineral of subgroups in which the cations are (a) Mg2+ + composition II, recently approved by the Comission on (b) Mg2++ Fe3+, and (c) Mg2++ Cr3+.The octahedral New Minerals and Mineral Names (CNMMN) of the environment of the cations is formed by hydroxyl International Mineralogical Association (no. 92-028 (OHt ions, whereas the interlayer voids are filled with [6]), should also be related to this subgroup. although (C03)2- anions and H20 molecules. The two modifica- the detailed mineralogical and structural data for this tions characteristic of these compounds are considered mineral have not been published. In relation to this, the as polytype 2H and 3R modifications with different unit mineral from the Jacupiranga alkaline-ultrabasic car- cell parameters a and c (in the hexagonal setting): 3.1 bonatite massif (Sao Paulo, Brazil), first described as and 15.6 Afor the former and 3.1 and 23.4 Afor the lat- manasseite [7] but, in fact, having a composition con- ter polytype. sistent with the data for a new representative of the sub- In the subgroup of (Mg, AI)-hydroxides of the com- group of the dihydroxides under consideration, is of positions Mg6AI2(OH)16(C03). 4H20 (I), the 2H poly- great interest, and the determination of its structure was type is manasseite and the 3R polytype is hydrotalcite; the main purpose of this study. in the subgroup of the (Mg, Fe) hydroxides having sim- ilar compositions, the 2H polytype is sjogrenite and the 3R polytype is pyroaurite. The corresponding minerals EXPERIMENTAL in the subgroup of (Mg, Cr)-hydroxides are stichtite The mineral under consideration was discovered in and barbertonite. The above compositions of natural the form of bright orange-red 2-6-mm large grains in and synthetic hydrotalcite [1-3] differ from the compo- dolomites [6]. The crystals had hexagonal trapezoidal sition established in the X-ray structure determination faceting, with prismatic faces and basal pinacoidal . 3H20 (II) [4]. of this mineral-Mg4AI2(OH)12(C03) faces, parallel to which perfect cleavage was observed. Hydrotalcite formulas 1 and II have different numbers X-ray single-crystal studies (a SYNTEX automatic dif- of C03 groups, the same numbers of (Mg + AI) cations, and different values of the Mg :Al ratio (3 : 1 for 1 and fractometer, sp. gr. PI, MoKa radiation) were per- 2 : 1 for II). formed on a O.025-mm-thick crystalline platelet witha @ 1063-7745/96/4106-0972$10.00 1996 MAMK Hayr<:a /Interperiodica Publishing CRYSTAL STRUCTURE AND COMPARATIVE CRYSTAL CHEMISTRY 973 Table1. Characteristics of the minerals of the hydrotalcite-manasseite subgroup according to different sources Sp. gr. or Chemical formula Unit cell parameters, References Mineral lattice type A HydrotaIcite AI2M&(OH)16C03 . 4H20 (I) R3m a = 3.102, C = 23.404 [2] AI2M&(OH)16C03 . 4H20 (I) R a = 6.142, C = 46.24 [8] AI2M~(OH)12C03 . 3H20 (II) R3m a =3.054, C =22.81 [4] Manasseite AI2M&(OH)16C03 . 4H20 (I) P63/mmc a=3.1,c=15.5 [1] AI2M&(OH)16C03 . 4H20 (I) H a = 6.13, c = 15.37 [9] Chlonnagaluminite AI2(Mg, FeMOH)12 . (Cl, (C03)O.5h . 2H2O P63/mcm a =5.29, c =15.46 [5] maximumdimension in the plane of 0.625 mm. The this space group up to the reliability factor R =0.12. twelvemost intense reference reflections provided the The model structure consisted of two brucite-type lay- establishmentof a hexagonal unit cell with the lattice ers perpendicular to the 63 axes, each of them being parameters a' = 3.050(1) and c = 15.150(9) A, which, built by three (Mg, Al)-octahedra (layer l' in Fig. 2a). togetherwith the data on the chemical composition, The 0 and C atoms are located between the layers at the indicatedthat the crystal belonged to the hydrotalcite- same height z (the 0 net in Fig. 2a). In addition to the manasseitesubgroup (Table 1).As is seen from Table 1, 6raxis, the brucite layers were also related by the plane thebasis parameters of the hexagonal unit cells can be m normal to this axis and passing through the (C, 0) chosen differently depending on the presence or nets and by the coordinate plane c absent in the initial absenceof a small number of weak reflections indicat- symmetry group. The interlayer nets related by the ingan increase in the minimum translation vector a': 6raxis and the c plane also had half-filled positions of (i)a = a' = 3.05 A, (ii) a = 2a' = 6.1 A, or (iii) a = C and 0 atoms of the C03 groups and H20 molecules. a' J3 = 5.28 A. There is another, fourth, possible vari- The 50% occupancy of the C-position lying at the inter- section of the 2 and 63 axes with the three 0 atoms ant of the translation, (iv) a = 2a' J3 = 10.56 A (Fig. 1). bound to it and also at the intersection of three 0 atoms To avoid any possible loss of experimental data, the from the H20 molecules followed from the chemical basic set of X-ray reflections was obtained for the unit composition of compound II and was confirmed by the cell with the maximum parameter, a = 2a'J3 = electron-density values on the F-synthesis for the 10.566 A, within half of the Ewald sphere (sinS/A. = model obtained. The identical interlayer nets allowed 0.81A-l). Altogether, 262 reflections with I > 2cr(I) us to describe the model within the sp. gr. P63/mcm, wererecorded. The analysis of their intensities indi- which was inconsistent with the presence of weak cated the diffraction class 6/ mmm. Upon averaging, the reflections not obeying the extinction rule imposed by experimental set contained 52 crystallographically independent reflections; the reliability factor for the 2a'J3 equivalent reflections was R =0.059 (over 39 groups of a = reflections). The absence of reflections with odd h and k indices indicated a parameter half as large, a = 5.283 A. a=a'J3 The attempt to ,.pass to the unit cell with the parameter a = 2a' = 6.01 A with the aid the matrix (2/31/30, -1/3 1/30,001) resulted in the loss of seven reflections; the remaining reflections had either even h or even k indi- ces. This indicated the presence of a pseudotranslation a' =3.05Aalong the [210] direction in the unit cell with the parameters a = 5.283(3) and c = 15.150(9) A. Weperformed a complete structure determination withinthis unit cell. All of the calculations were per- formedusing the AREN program complex [10] taking into account anomalous atomic scattering. Structure amplitudes were calculated from the intensities with dueregard for the polarization and Lorentz factors. b = 2a'J3 The regular extinctions in the intensities of the (0001)reflections with I =2n + 1 within the diffraction Fig. 1. Relationship between the a vectors of the hexagonal class6/mmm indicated the space group P6322. A struc- unit cells in the structures of various minerals of the ture model was determined by direct methods within dihydroxide group. CRYSTALLOORAPHY REPORTS Vol. 41 No.6 1996 974 ARAKCHEEV A et ai. two threefold axes, in accordance with chemical for- mula n. A high value of the thermal parameter of the C atom (> 10 A2) indicated possible splitting of its posi- tion. The F-synthesis provided the localization of the peak lying at a distance of 0.3 A from the initial posi- tion of the C atom (and from the m plane) along the z-axis. Thus, we placed this atom into this position with 50% occupancy. The refinement of the split C-position reduced the reliability factor down to R =0.055 and the thermal parameter down to 6.0 A2.
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